5-Pyrimidinol, 4-amino-6-chloro- (9CI) synthesis

Yield: 85%

Reaction Conditions:

Stage #1:6-chloro-5-methoxypyrimidine-4-amine with boron tribromide in dichloromethane at 20; for 72 h;
Stage #2: in methanol;dichloromethane at 20; for 2 h;

Steps:

83 Synthesis of 4-amino-6-chloro-5-ol
Dissolve 6-chloro-5-methoxypyrimidin-4-amine (5.5g, 34.6mmol) in dichloromethane (50ml), slowly add boron tribromide (11ml) dropwise, and complete the reaction at room temperature for 72 hours. Methanol (100ml) was added, stirred at room temperature for 2h, concentrated in vacuo, and the residue was separated by silica gel chromatography (developing solvent: petroleum ether: ethyl acetate=1:1) to obtain a gray solid (4.26g, 85%).

References:

China Pharmaceutical University;Chen Yadong;Lu Tao;Cui Bingbing;Jiao Yu;Tang Weifang;Fan Lu CN112047932, 2020, A Location in patent:Paragraph 0453-0456